chlorine determination
TRANSCRIPT
RESEARCH AND DEVELOPMENT BULLETIN RD082T
Coal Characterization by X-Ray Spectrometry
\ by J. L. Bernardi
PORTLAND CEMENT ASSOCIATION Research and Development/Construction Technology Laboraforres
- Coal Characterizationby X-Ray Spectrometry
certified analysis. Chloride, sulfur, ash,and caloriflc values were determined onthe whole coal samples. Mineral analy-ses of the ash were also carried out onfour of the coals. Following is a discus-sion of the results.
by J. L. Bernarcji’PROCEDURES
BACKGROUND
Coal as a kiln fuel was used in 86% oftotal production in the U.S. cementindustry in 1980, and its use is still in-creasing. Kiln system buildups andquality control problems have becomemore prevalent as this rapid conversionto coal-fired cement kilns has takenplace.
Chlorides are frequently present incement feed materials in an amount thatgenerally does not exceed 0.01% to0.02Y0. This concentration usually doesnot cause buildup problems in preheaterkiln systems. Many coals, however,have much higher chloride contents andsuch coals can contribute to preheater
n problems. In fact, coal may often beconsidered the predominant source ofchloride during clinker production;thus, it is highly desirable to develop arapid, accurate method 10 determine thechloride content of coal.
The composition of tlhe coal ash alsomust be known since most of the ash isincorporated into the cement clinker. Inorder to produce a material of consist-ent high quality, adjustments must bemade continually in th[: feed materialsas a function of both the amount andthe chemical composition of the ash.Therefore, it is important to develop arapid, accurate method to determine themajor oxide contents of whole coal.
Analysis of whole coal for majoroxides by wet methods or atomic ab-sorption is a lengthy procedure thatcould require several days. Using X-rayfluorescence spectrometry, the wholecoal sample can be ground, pressed, andanalyzed for 10 oxides and chloride inless than two hours.
EQUIPMENTm
Samples were analyzed with a memory-controlled, automatic sequentialRigaku Model 3064 X-ray vacuum
spectrometer. The spectrometer’s cen-tral controller memorizes and controlsa large number of optimized measure-ment conditions. The analyzing cham-ber contains a vertically mounted, rho-dium-target, end-window X-ray tubewith the target face parallel to the sam-ple surface. This close coupling of thetarget with the sample surface and theuse of a very thin beryllium window inthe X-ray tube provide optimum excita-tion of the elements above atomic num-ber 8 with a single tube.
During each X-ray fluorescence run,the X-ray intensities of five sampleswere measured by the spectrometer andrelated to a standard for a sequence of10 elements: silicon (Si), aluminum (Al),iron (Fe), calcium (Ca), magnesium(Mg), sulfur (S), sodium (Na), potas-sium (K), phosphorus (P), and titanium(Ti). No background corrections weremade. The instrumental parametersare listed in Table 1. Chloride intensitieswere measured separately as only 10elements can be analyzed sequentiallyon the Rigaku X-ray spectrometer.
SAMPLES
Samples used in this study were ob-tained from Alpha Resources, Inc.(’)**Each sample was prepared in accord-ance with American Society for Testingand Materials (ASTM) Designation:D2013 and sealed in amber bottlesunder an inert atmosphere. Each sam-ple was supplied with a certified analy-sis that stated the proximate analysis,ultimate analysis, sulfur forms, mineralanalysis of the ash, and ash fusion tem-peratures. A total of 22 samples wereused to prepare the X-ray fluorescencecalibration curves for whole coal. Typesof whole coals studied are listed in Table2A and certified analyses of these wholecoals are summarized in Table 2B.
Several of the 22 samples were ana-lyzed to determine the reliability of the
Chloride
Chloride analyses were made for ninesamples per ASTM procedure D2361and are summarized in Table 3. In theASTM method the sample was mixedwith an Eschka mixture (two parts mag-nesia and one part sodium carbonate)and ignited in a Parr adiabatic calorim-eter. The fused product was dissolvedin hot water, acidified, and analyzed byeither the Volhard method or poten-tiometric titration. The Volhard meth-od was used by most of the laboratoriesanalyzing these samples for certifica-tion, but it can give rise to significanterrors at these low concentrations. Apotentiometric titration using a silversulfide ion-selective electrode is usuallyan extremely accurate method to deter-mine low levels of chloride.
The analytical laboratory at PCA hasdeveloped a potentiometric method todetermine chloride ‘7) in cement, lime-stone, clay, and so forth, usually withan accuracy of plus or minus 0.00290 to0.003qo. Nine coal samples were repeat-ed two to five times each, and the aver-age value for each sample was used tomake up the X-ray fluorescence calibra-tion cu~ve. Table-3 shows that the certi-fied values for samples AR 219 and AR774 had significant errors. A later certi-fication sheet, received after this analy-tical work was completed, reduced thechloride level from 0.06% to 0.0570 forAR 774, and this corrected value (O.05%)is the one listed in Table 3.
Sulfur
Sulfur analyses were determined induplicate or triplicate on 10 of the whole
*Former Senior Research Chemist, ProcessDevelopment Section, Chemical/ Physical Re-search Department, Portland Cement Associa-tion, Skokie, Illinois.
**Superscript numbers ,n parentheses denote
references at the end of this text.
@ portland cerne~t Association 1982
2 Coal Characterization b-y X-Ray Spectrometry
coals, according to ASTM procedureD3177. In this method, the sample wasignited in a Parr bomb and sulfur wasdetermined gravimetrically as sulfatefrom the bomb washin{;s. Results aresummarized in Table 4. These valuesagreed well with the certified results;therefore, the certified values were usedfor the calibration curve. (Certifiedvalues for sulfur were converted to sul-fur trioxide by multiplying by a factorof 2.5.)
Calorific Value
Calorific values were determined on 12samples following ASTM methodD2015 and are summarized in Table 5.Samples AR 114, 216, 217, 218, 219,and 220 were run two weeks to twomonths after the bottles containingthem were opened. Seve~-al members ofASTM Committee D5 recommendedthat heating value determinations berun within a week of preparation (grind-ing), otherwise low results could be ex-pected; in fact, low results were obtainedfor each of these samples. Later sam-ples (AR 213, 774, 778, 779, 780, and782) were analyzed immediately aftersealed bottles were opened, and all re-sults were within ASTM limits.
Ash
Ash analyses were run on 10 coal sam-ples according to ASTMIMethodD3174with some modifications. Instead ofusing a l-g sample in a porcelain cruci-ble, a 10- to 20-g sample of each wholecoal in a porcelain evaporating dish wasused. Approximately 2 g of ash wereproduced by this proceclure, so that acomplete chemical anallysis could becarried out on the ash. The sample washeated to 500° C in abolut one hour toexpel the volatiles from the coal, thentaken up to 750° C and kield there for aminimum of one to two hours. The re-sults, listed in Table 6, are all withinASTM limits.
Lignites and subbituminous coals aresometimes high in lime and may retainmuch of the sulfur in the coal. Most ofthe sulfur in whole coal is evolved as sul-fur dioxide when heatt:d to between250° C and 350° C. A rapid tt?mperaturerise in this range will result in sulfur di-oxide loss and the combined calciumsulfate will be low. For these samples itis especially important to follow pre-
cisely the ASTM ashing procedures toobtain the correct ash value.
Ash Analyses
A complete ash analysis was carried outon four ash samples (AR] 14, AR 218,AR 219, and AR 220) by PCA’S analy-tical staff. Each ash was fused withlithium metaborate (L.iBOZ) and ana-lyzed by atomic absorption spectrom-etry, following the same meth(~~ds usedat PCA to analyze cement. “ Phos-phorus pentoxide was determined col-orimetrically(~) by a PCA molybdenumblue method. Ash analyses were con-verted to a whole coal basis and aresummarized in Table ‘7.
In most cases the agreement was suf-ficient to justify using the certified anal-ysis to determine oxide concentrationsfor the calibration curves. Results forsodium oxide and potassium oxide wereslightly higher than the certified results.ASTM method D3682 uses a lithiumtetraborate (LiB,O,) fusion at 1000° Cwhile PCA’S cement method uses a lith-ium metaborate (Li BO~) fusion at900° C. The higher ASTM fusion tem-perature may volatilize more of theNa~O and KzO and give lower results.PCA results for Na~O averaged about0.0 1% higher and for KzO about 0.02%higher. However, these differences werenot considered significant enough towarrant correcting. l-he phosphoruspentoxide results were much lower andare discussed below.
The percentages for silica (SiOz),alumina (AljO~), ferric oxide (FejO~),lime (CaO), magnesia (MgO), sodiumoxide (Na~O), potassium oxide (KZO),phosphorus pentoxide (P~Os), andtitania (TiO~) used in the calibrationcurves were determined by multiplyingthe decimal percentage of the oxide inthe mineral analysis by the percentageof ash in the sample.
Phosphorus Pentoxide
Phosphorus pentoxide was measured in10 of the whole coal samples using thePCA method(~) for determining its con-tent in cement. Iron does not interferewith this method but does interfere withthe ASTM D3682 method for Pz05 incoal. Initial plots using the certifiedvalues for Pz05 gave an elliptical curveinstead of a straight line. Alpha Re-sources confirmed that their PZOS re-
sults were not reliable and that they _were trying to develop a better method.
At the October 1980 ASTM Commit-tee D 5 meeting, it was brought out thatthe coal ash fusion melt samples shouldbe digested in 10% nitric acid (HNO~)instead of 5~0 hydrochloric acid (HC1).Chloride forms the ferric chloride(FeCl~ ) complex with the ferric ion,which is bright yellow in color; this ironcomplex enhances the P?O~ concentra-tion in the calorimetric determination.
During 1980, Alpha Resources re-ceived results from another laboratoryusing several independent methods fordetermining PzO~ that were in goodagreement with PCA’S results. There-fore, PCA’S results listed in Table 8 wereused for the P~O~ calibration curve.
SAMPLE PREPARATION
Reagents and Apparatus
1. Somar mix’X} or Chemplex X-raymix”]
2. Tungsten carbide grinding cell andBleuler mill
3. 30-mm-diameter aluminum cup z(Chemplex Cat. No. 500)
4. Evacuable X-ray die (Spex. Cat.No. 3623)
5. Compression machine capable of41,000-lb load
6. Vacuum pump
Procedure
1.
2.
3.
4.
5.
Four and one-half grams of driedcoal or coal char and 1Ag of Somarmix were ground for 4 minutes in atungsten carbide cell of the Bleulermill.The ground material was brushedout of the cell onto a clean piece ofsmooth-surfaced paper. An alumi-num cup was filled with the powderand placed inside the bore of thebriquetting die assembly. The re-maining powder was poured intothe bore on top of the aluminumcup.The sample on the surface of thecup was uniformly distributed bycarefully inserting the plunger andholding it against the sample.The plunger was slowly withdrawnso as not to disturb the distribution ~of the sample.A steel pellet was placed in the bore
PCA Research and Development Bulletin 3
6.
7.
8.
9.
10.
11.
I2.
with its polished side downwardand then gently pressed down withthe plunger.The die assembly was completedby placing the top O-ring aroundthe plunger.The assembly was brought to thecompression machine and thevacuum line connected to the pipeprotruding from the die. The vacu-um pump was then started.Slowly a load was applied on theassembly, bringing the load to 3000lb. This load was hf:ld for M minuteto remove entrapped air.The load was gradually increasedto 40,000 lb, maintained there for1 minute, brought up to 41,000 lb,and then released.The vacuum line wi~s disconnected,the assembly inverted, and its baselifted off.The Perspex ring supplied with thedie assembly was placed on top ofthe cylinder and tlhe assembly re-placed in the press.A load was applied to the assem-bly for the plunger to lift the pelletsand sample briquet out of the bore.
Notes on Procedurf:
1. Four minutes of grinding in theBleuler mill eliminated the influ-ence of the particle size of the coalsample on X-ray intensity.
2. It was also found tlhat a pelletizingpressure of 40,000 lb assured ob-taining stable and reproducibleX-ray intensities.
3. Somar mix is a pure organic com-pound that is used as a binder. Afew coals and coal chars cannot bepelletized without using a binder.Chemplex X-ray mix may be usedinstead of Somar mix.
MATHEMATICAL TREATMENTOF DATA
Linear regression was carried out ondata for each oxide, using measured rel-ative intensities and cah:ulated percent-ages of oxide on the whole coal basis.The correlation factor (r). slope, andintercept were calculated for each oxideand are summarized in ‘Table 9. Results
n for MgO, NaZO, PzO~, TiO~, and KzOwere generally acceptable. Results forSiO~, AIzOS, and CaO were acceptable
only if one or more lignite and sub-bituminous samples were eliminatedfrom the linear regression.
Linear regression proved unsatisfac-tory for Fe,O, and SOS. These oxideswere run by the multiple regressionequation developed by Lucas-Toothand Pyne. (4 s) This eql~ationmade cor-
rections for absorption and enhance-ment effects and used X-ray fluorescentintensities, which can be measured ex-perimentally, rather than oxide con-centrations, which must be known orestimated in other formulations such asthat of Heinrich. The Lucas-Tooth andPyne equation requires a large numberof standards. In this approach, ninevariables (~11- ~g) have to be determinedfrom a series of simultaneous equa-tions (one for each standard) and abouttwice that number of standards (15 to20) are required to evaluate these vari-ables. P() is a constant and ~1 through 6Xare influence coefficients of one elementon another element. For FeZOS theequation has the form:
where Cp.zoj is the weight percentageof Fe~O~ in the sample and [F’?201 is the
intensity of iron, IS,(J7is the intensity ofsilicon, and so forth.- All intensities arein counts per second.
This equation contains nine variablesthat were evaluated using an IBM step-wise linear regression program(c] on aDigital Scientific computer. Equationssimilar to that above can be written andevaluated for each of the oxides. Thecoefficients for the equations are sum-marized in Table 10. ~iOl, Al~O~, KzO,and TiO~ were also evaluated using thisprocedure.
The intensity of each oxide was deter-mined by dividing the total X-ray countsby the count time. The counts per sec-ond ranged from several hundred forCaO to sixty thousand for Fe,O~ andSO,. For computing purposes, all countswere coded by dividing by 1000. Allnumbers were rounded to the nearesthundredth. The raw data for the multi-ple regression are summarized in theAppendix.
DISCUSSION OF RESULTS
Sulfur Trioxide
Sulfur trioxide (S0,) is the most diffi-cult of the 10 oxides to analyze by X-rayfluorescence. Linear regression using all22 samples gave a standard deviation of0.5590 and multiple regression gave astandard deviation of 0.38’% (see Tables11 and 12). These standard deviationsare much too high for acceptable analy-tical results.
Examination of the sulfur concentra-tion showed that 15 of the coals had lessthan 5. 15% SOI. A second set of multi-ple regression coefficients was generat-ed using these 15 samples (see Table 10).It gave a correlation factor of 0.9892, astandard deviation of O.17Y0, and anaverage error of O. 14Y0. Nine of thesesamples were within ASTM limits (seeTable 13). For samples with under 2%sulfur, ASTM calls for a repeatabilityof 0.05Y0, which corresponds to O.13%for samples containing less than 570SO~. The coefficients for all 22 coals (seeTables 10 and 12) gave an average errorof 0.28Yo; for the 15 samples with SOJcontents less than 5. 15%, only four (AR771, 774, 775, and 778) are withinASTM limit of O.13Y0.Coefficients list-ed in Table 10 for S07 (low) should givereasonably good analytical data forsamples containing less than 5.1570 SOI(or 2.06% sulfur). Multiple regressionanalysis was not made for high SO~levels (greater than 5. 1570) because sev-eral more samples would be required todetermine the regression coefficients.
Silica and Alumina
Both silica (SiOZ) and alumina (AIzOS)were evaluated by linear and multipleregressions (see Tables 14 through 17).In both cases the multiple regressionresults for whole coal analysis were ac-ceptable. Linear regression results wereacceptable for silica when the lignite(AR 777) and two subbituminous sam-ples (AR 215 and AR 773) were not in-cluded in the regression analysis, andfor alumina when the lignite sample(AR 777) was not included.
Ferric Oxide
Linear regression for ferric oxide(FezO~) was unsatisfactory. The lignitesample (AR 777) and the two subbitumi-
4 Coal Characterization by X-Ray Spectrometry
nous samples (AR 215 and AR 773)were not used. The linlear regressiongave a standard deviation o10.28% andan average error of 0.229.; more thanhalf the samples had errors exceeding0.20%. Multiple regression using all 22samples gave a standard deviation of0.1 IYo, an average error of 0.08%, andonly one sample error exceeding 0.20T0(see Tables 18 and 19).
Lime
Linear regression could be used for lime(CaO) if the lignite sample (AR 777) andtwo subbituminous samples (AR 215and AR 773) are not used, but it is notvery satisfactory. It gave both an aver-age error and a standard deviation of0.05%. Multiple regression using all 22samples gave a more accurate analysis,reducing both values to 0.02% (see Ta-bles 20 and 21).
Magnesium Oxide
Linear regression results for magne-sium oxide (MgO) were not particularlysatisfactory, but the errors were not sig-nificant in that only one sample con-tained more than O.18% ltigo (see Table22). Results may be improved if the twosubbituminous samples are not includ-ed in the linear regression computation.
Potassium Oxide andTitanium Dioxide
Potassium oxide (KJC~) and titania(TiO~) could be analyzed by eitherlinear or multiple regression. For bothoxides, multiple regression gave a moreaccurate analysis (see Talbles 23 through26). Improved results may be obtainedif the lignite sample is eliminated fromthe linear regression for both K,O andTiOZ.
Sodium Oxide
Linear regression results for sodiumoxide (NaqO) were acceptable eventhough there is a difference of 0.3% be-tween the two subbituminous samples(AR 215 and 773) and the 20 other sam-ples (see Table 27).
Phosphorus Pentoxide
Linear regression gave satisfactory re-sults for phosphorus pentoxide (PzOS)on the 10 samples that were analyzed(see Table 28). The Pz05 concentrations
were all less than 0.06q0 and no errorexceeded 0.0 Ioz,.
Chloride
Linear regression data for chloride inwhole coal (Table 29) showed that thecorrelation factor was very close to one,the standard deviation 0.004Y0, and theaverage error 0.003Y0. Therefore, chlo-ride can be determined very accuratelyby X-ray fluorescence. Extreme caremust be exercised not to touch the sur-face of the pellets, as salt deposited onthe pellets will increase chloride resultssignificantly.
Coal Samples
Table 2B shows that four cokes and 13bituminous, one anthracite, one lignite,and three subbituminous coals wereused in this study. The subbituminous(AR 215, AR 510, and AR 773) and lig-nite (AR 777) samples often gave un-satisfactory results. Other analysts havealso reported problems with these typesof samples, apparently because thesecoals have a different matrix, moisturecontent, and density. This may explainsome of the difficulty in utilizing thesesamples in linear regression analyses.
CONCLUSIONS
1. This study has shown that it is pos-sible to determine the 10 major oxidesin whole coal rapidly and accuratelyby X-ray fluorescence.
2. Bituminous coals and cokes gave ac-ceptable results. Unsatisfactory re-sults were often obtained for linearregression calculations using the lig-nite sample from Texas (AR 777) andthe two subbituminous samples fromWyoming (AR 215 and AR 773);however, multiple regression resultsusing these samples were acceptable.A third subbituminous coal (AR 5 10)from the Texas-Oklahoma bordergave satisfactory results. Only oneanthracite sample (AR 776) wasavailable for inclusion in this studyand it also gave satisfactory results.
3. Chloride also can be determined ac-curately and rapidly by X-ray fluo-rescence.
4. Matrix corrections are required forsulfur trioxide (SO~) and ferric oxide(Fe~O~). Even with matrix correc-
5.
tions, the SO, results were not very _satisfactory. However, acceptableresults were obtained when matrixcorrections were applied only to thosecoal samples that contained less than5. 15% SO,. More coal samples wouldbe needed to determine if acceptableresults could also be obtained forthose coals with SO? levels greaterthan 5. 15Y0.
Matrix corrections may also improveresults for silica (SiOz), alumina(A1,O,), lime (CaO), potassium oxide(KzO), and titania (TiO~), especiallyif lignite and subbituminous samplesare used.
REFERENCES
1. Alpha Resources, Inc., P.O. BOX199, Stevensville, Michigan 49127,(616) 465-5559.
2. Crow, R. F., “Atomic AbsorptionAnalysis of Portland Cement, Clink-er. and Raw Mix Using Lithium
3.
4.
5.
6.
7.
M’etaborate Fusion,” Tes~ !dethodsof the PCA Analytical ChemistrvLaboratories, Portland CementAssociation, 1980, pages 2.1-21. nMivelaz, W. F., and LaBonde, E. G.,“Determination of Percent Phos-phorus and Titanium in PortlandCement, Clinker, Kiln Feed, andRaw Materials by Means of the GoldCrucible and Sodium Hydroxide (orLithium Metaborate) Fusion Meth-od.” Unpublished PCA procedure.E. P. Bertin, Principles and Practicesof X-Ray Spectrometric Anal.vsis,2nd Edition, New York-London,Plenum Press, 1975, page 685.Lucas-Tooth, J., and Pyne, C., “TheAccurate Determination of MajorConstituents by X-Ray FluorescentAnalysis in the Presence of LargeInterelement Effects,” Advances inX-Ray Analysis, Vol. 7, New York,Plenum Press, 1964, pages 523-541.IBM Application Program 1130 Sta-tistical System (11 30-CA-06X).Bernardi, J. L., and LaBonde, E. G.,“Determination of Chloride in Ce-ment Fuels and Raw Materials,”PCA R&D Ser. 1668 (198 1). To bepublished.
8. Somar Laboratories, 54 East 1IthStreet, New York, New York 10003.
9. Chemplex X-Ray Mix, Chemplex nIndustries, Inc., 34 Bradley Road,Scarsdale, New York 10583.
)TA
BLE1.
X-Ra
yPa
rame
ters
forWh
oleCo
alAn
alys
is
E1eme
nt
Sili
con
(Si)
Alum
inum
(Al)
Iron (Fe)
Calc
ium
(Ca)
Mane
sium
?)Mg
Sulf
ur(s
)
Sodi
um(N
a)
Pota
ssiu
m(K
)
Phos
phor
us(P
)
Tita
nium
(Ti)
Chlo
rine
(cl)
Anal
yte
Crys
tal
line
EDDT
Ku
EDDT
K~
LiF(
200)
Ka
LiF(
200)
‘B
AOP
Ka
GeKa
TAP
Ka
LiF(
200j
Ka
GeKa
LiF(
200)
Ka
GeKa
Dete
ctor
FPC
FPC
Sc FPC
FPC
FPC
FPC
FPC
FPC
FPC
FPC
PHS
wind
ow
1-1
I-T
1-1
2-2
1-1
1-1
2-2
i-i
1-1
1-1
2-2
Coun
ting
time
(see
)
40 40 20 40 200 20 200 ?0 40 40 40
Abso
rber
1 ~ 1/2
1 1 1 1 i 1 1 1
Othe
rpa
rame
ters
were
:40
kV,70
ma,Rh
tube
,va
cuum
,1s
tor
der,
25-n
mIco
pper
mask
over
samp
le,sp
in,an
d0.
05sc
fhP-
10ga
sfl
owfo
rFP
C.
Slit
s
3s 3s 3s 3s 3s 3s 3s 3s 3s 3s 3s
)TA
BLE2A
.Co
alSa
mple
s
Samp
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
Desc
ript
ion
Coke
Coke
Subb
itum
inou
sfr
omWy
omin
gWe
stVi
rgin
iabi
tumi
nous
West
Virg
inia
bitu
mino
us
West
Virg
inia
bitu
mino
usAm
axbi
tumi
nous
Sout
hern
Amax
bitu
mino
usSo
uthe
rnIl
lino
is/I
ndia
naIl
lino
is/I
ndia
naSo
uthe
rnIl
lino
isbi
tumi
nous
Subb
itum
inou
sOk
laho
ma-T
exas
bord
er
Coke
Coke
Subb
itum
inou
sfr
omWy
omin
gKe
ntuc
kybi
tumi
nous
Kent
ucky
bitu
mino
us
Penn
sylv
ania
anth
raci
teLi
gnit
efr
omTe
xas
Nort
hwes
tVi
rgin
iabi
tumi
nous
Ohio
bitu
mino
usSo
uthe
rnIn
dian
abi
tumi
nous
Sout
hern
Illi
nois
bitu
mino
usSo
uthe
rnIl
lino
isbi
tumi
nous
TABL
E2B
.Ce
rtif
iedVa
lues
forSt
anda
rdWh
oleCo
alSa
mple
sm
(Sou
rce:
Alph
aRe
sour
ces,
Inc.
)
Thefo
llow
ingAS
TMpr
oced
ures
were
empl
oyed
inth
ean
alys
isof
allsa
mple
s:
Prep
arat
ion
ASTM
D201
3-72
(78)
Vola
tile
Matt
erAS
TMD3
175-
77
Ash,
%Vo
lati
le,%
Fixe
dca
rbon
,%
Btupe
rpo
und
Sulf
ur,%
Chlo
ride
,%
Phos
phor
uspe
ntox
ide
(P~o
~)Si
lica
(Si0
2)Fe
rric
oxid
e(F
e203
)Al
umin
a(A
1203
)Li
me(C
aO)
Magn
esia
(MgO
)Su
lfur
trio
xide
(S03
)Po
tass
iumox
ide(K
20)
Sodi
umox
ide(N
a20)
Tita
nia(T
i02)
Unde
term
ined
Coke
AR11
4
9.85
1.86
88.2
913
,024
0.91
0.05
0.44
52.6
09.
7929
.10
2.46
0.79
0.86
1.70
0.39
1.44
0.43
Sulf
urAS
TMAs
hCo
nten
tAS
TM
Coke
AR21
3
6,88
3.57
89.5
512
,622
0.60
0.04
0.71
50,2
914
.63
26.0
01.
450,
920.
052.
340.
371.
611.
63
Coal
~21
5
5.66
40.3
753
.97
12,3
770.
460.
03
D317
7-75
AshAn
alys
isAS
TMD3
682-
78D3
174-
73(79)
Chlo
rine
ASTM
D236
1-66
(78)
Prox
imat
ean
alys
is(d
ried
basi
s)
Coal
Coal
Coal
AR21
6AR
217
AR21
8
7.51
10.4
78.
2625
.08
36.5
938
.81
67.4
152
.94
52.9
314
,439
12,8
6913
,513
0.99
1.23
2.56
0.20
0.03
0.20
Mine
ralan
alys
is(w
eigh
t,%,
igni
tedba
sis)
0.75
0.46
30.0
050
.20
6.19
9.07
16.4
030
.00
15.6
42.
653.
220.
6616
.40
2.33
0.42
1.53
7.92
0.51
1.12
1.58
1.94
1.01
0.63
55.8
09.
1426
.60
1.11
0.68
0.67
1.98
0.24
1.24
1.91
0.78
39.2
025
.42
21.4
03.
411.
164.
021.
920.
361.
261.
07
Coal
AR21
9
14.1
037
.60
48.3
012
,233
3.70
0.02
0.72
44.3
025
.32
18.9
03.
260.
623.
471.
470.
290.
990.
66
Coal
AR22
0
lo.m
43.0
346
.97
12,8
764.
320.
01
0.87
44.5
029
.59
18.8
00.
930.
740.
682.(
?00.
140.
990.
76
Btu
Coal
AR38
0
12.8
439
.00
48.1
612
,412
3.62
0.03
0.61
38.7
021
.91
17.7
97.
980.
829.
011.
810.
380.
760.
23
Coal
AR51
0
10.6
738
.69
50.6
412
,421
5.08
0.04
0.29
29.9
549
.M16
.25
0.75
0.41
1.01
1.24
0.30
0.73
0.03
6.82
* fb2.
82n T
90.3
6;
13,5
522
0.59
k
0.03
0.52
49.1
514
.62
26.0
81.
530.
930.
882.
400.
471.
621.
80
)
))
TABL
E2B
.(C
onti
nued
)
Ash,
%Vo
iati
ie,%
Fixe
dca
rbon
,%
Btupe
rpo
und
Sulf
ur,%
Chlo
ride
,%
Phos
phor
uspe
ntox
ide
(p20
5)Si
lica
(Si0
2)Fe
rric
oxid
e(F
e203
)
Alum
ina(A
1203
)Li
me(C
aO)
Magn
esia
(MgO
)Su
lfur
trio
xide
(S03
)Po
tass
iumox
ide(K
20)
Sodi
umox
ide(N
a20)
Tita
nia(T
i02)
Unde
term
ined
Coke
AR7?
2
8.B8
.1.
1.11
90=(
!112
,737
0.83
0.04
0.49
49.8
712
.46
27.4
22.
840.
882.
121.
820.
571.
350.
18
Coal
M77
3
5.47
.,A,
-41
.Y3
52,5
8
12,1
830.
390.
01
0.59
27.6
85.
9115
.94
14.2
33.
0723
.38
0.51
7.56
1.01
0.12
Coal
m77
4
7.21
5.n,
-J>
.YD
56
.83
13
,97
0
0.6
3
0.0
5
0.20
57.6
210
.62
19.9
23.
421.
292.
372.
420.
761.
000.
38
Prox
imat
ean
alys
is(d
ried
basi
s)
Coal
Coal
Coal
AR77
5AR
776
m77
7
6.55
11.0
123
.91
“r..
L3.DL
Fn.r
3C.4
3“n
““*U
.ZJ
~7
=8
336
.54
35,~
~
14,6
1614
,512
9,37
90.
891.
291.
410.
140.
070.
01
Mine
ralan
alys
is(w
eigh
t,%,
igni
tedba
sis)
0.42
0.21
0.29
48.2
842
.45
11.5
611
.14
29.1
924
.93
3.33
6.89
0.68
1.82
3.01
7.63
1.43
1.87
0.21
1.07
1.64
1.13
0.25
0.86
51.0
18.
8318
.30
8.42
1.96
8.74
0.92
0.23
1.06
0.24
Coal
AR77
8
7.74
.6..
J3.3
L56
,74
13,8
581.
430.
12
0.48
50.9
814
.47
24.6
82.
760.
762.
121.
630.
551.
170.
40
Coal
AR77
9
7.47
-C>.
-Jo
.13
56,3
814
,118
1.60
0.01
0.18
47.4
321
.78
22.0
11.
580.
991.
292.
740.
470.
800.
73
Coal
~78
0
8.22
mfi“r
JO.*
>53
.33
12,6
942.
060.
03
0.45
40.8
931
.92
19.2
51.
260.
791.
102.
050.
300.
971.
02
Coal
AR78
1
12.5
8.-
.,-.
JY.
>Y
47.8
3
12,5
232.
900.
01
0.32
53.9
516
.93
20.2
11.
351.
081.
182.
950.
571.
080.
38
COal
AR78
2
6.03
.-.-
+3.LU
48,6
9
13,6
253.
180.
01
0.39
34.9
236
.85
20.4
02.
500.
502.
180.
980,
310.
710.
26
TABL
E3.
Chlo
ride
inWh
oleCo
alCo
mpar
ison
ofPC
Ave
rsus
Alph
aRe
sour
cesAn
alys
es
Samp
le
AR11
4
AR21
3
AR21
6
AR21
7
AR21
8
AR21
9
AR22
0
AR77
4
AR77
8
(wei
ght,
%)
PCAAn
alys
es
PerAS
TMD2
361*
Aver
age
n,Q
45,
0.04
80.
046
0.04
6
0.03
7,0.
038
0.03
8
0.19
6,0.
195,
0.19
60.
198,
0.19
5,0.
195
0.02
8,0.
030
0.02
9
0.19
8,0.
201,
0.20
00.
200
0.02
9,0.
038,
0.03
20.
032,
0.03
0
0.01
3,0.
009
0.01
1
0.04
620.
044
0.04
60.
047
0.11
7,0.
117
0.11
60.
116,
0.11
4
Cert
ifie
d(A
lpha
Reso
urce
s)
0.05
0.04
0.20
~o.0
5
0.03
~o.o
l
0.20
:0.0
4
0.02
:0.0
1
0.01
:0.0
05
0.05
**
0.12
TABL
E4.
Sulf
ur(a
sS)
inWh
oleCo
alw
Comp
aris
onof
PCAve
rsus
Alph
aRe
sour
cesAn
alys
esQ
Samp
le
AR11
4
~~p~
~
AR21
6
AR21
7
AR21
8
AR21
9
AR22
0
AR77
4
AR77
8
AR77
9
(wei
ght,
%)
PCAAn
alys
es
PerAS
TMD3
177
0.88
,0.
89
0.50
,0.
59
0.96
,0.
97,
0.98
,0.
99
1.23
,1.
24
2.49
,2.
46,
2.51
3.69
,3.
73
4.28
,4.
25
0.60
,0.
60
1.43
,1.
45
1.54
,1.
55
Aver
age
0.89
0.60
0.98
1.24
2.49
3.71
4.27
0.60
1.44
1.55
Cert
ifie
d(A
lpha
Reso
urce
s)
0.91
0.50
0.99
~o.0
4
4.32
~0.D
7
0.63
1.43
1.60
*Usi
ngpo
tent
iome
tric
titr
atio
npr
oced
ure.
**Co
rrec
tedva
lue;
earl
ierce
rtif
icat
ionli
sted
as0.
06%.
)
)TA
BLE5.
Calo
rifi
cVa
lues
forWh
oleCo
alCo
mt)a
riso
nofPC
Ave
rsus
Alph
aRe
sour
cesAn
alys
es
)TA
BLE6.
Ash
inWh
oleCo
alCo
mpar
ison
ofPC
Ave
rsus
Alph
aRe
sour
cesAn
alys
es
Sam
ple
AR11
4
AR21
3*
AR21
6
AR21
7
AR21
8
AR21
9
AR22
0
AR77
4*
AR77
8*
AR77
9*
AR78
0*
AR78
2*
(Bri
tish
ther
malun
itspe
r
PCAAn
alys
es
PerAS
TMD2
015
Aver
age
12,8
95;12
,895
12,8
95
13,6
18;13
,588
13,6
03
14,3
7114
,371
12,7
7512
,775
13,4
43;13
,428
13,4
35
12,1
60;12
,170
;12
,155
12,1
34
12,7
4512
,745
13,9
19;13
,931
13,9
25
13,8
74;13
,862
13,8
68
14,1
22;14
,088
14,1
05
12,6
8812
,688
13,6
5413
,654
poun
d)(w
eigh
t,%)
Cert
ifie
d(A
lpha
Reso
urce
s)
13,0
24
13,6
22
14,4
3935
5
12,8
69~6
3
13,5
1326
2
12,2
3324
4
12,8
76~3
8
13,9
70
13,8
58
14,1
18
12,6
94
13,6
25
Samp
le
AR11
4
AR21
3
AR21
6
AR21
7
AR21
8
AR21
9
AR22
0
AR77
4
AR77
8
AR77
9
PC
AA
nal
yses
Per
AS
TM
D31
74Mo
difi
ed
9.70
,9.
63
6.87
7.52
10.4
7,10
.51
8.21
,8.
13
14.2
2,14
.17
10.0
9,10
.00
7.18
7.67
7.42
Cert
ifie
d(A
lpha
Reso
urce
s)
9.85
6.88
7.51
~0.2
8
10.4
7:0.
33
8.26
~0.2
9
14.1
0:0.
41
10.0
0:0.
30
7.21
7.74
7.47
~res
hly
open
edbo
ttle
s.
TABL
E7.
AshAn
alys
isCo
nver
tedto
Whol
eCo
alBa
sis
Comp
aris
onof
PC
Ave
rsu
sA
lph
aR
eso
urc
esA
nal
yses
Si02
AlO
23
FeO 23
CaO
MgO
Na20
K20
P205
Ti02
PCAAn
alys
es~e
r~~f
~e~
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
esCe
rtif
ied
PCAAn
alys
es(C
erti
fied
)*Re
vise
dAR
**
PCAAn
alys
esCe
rtif
ied
(wei
ght,
%)
AR11
4
5.10
KIQ
Q.r
”
2.80
2.87
0.98
0.96
0.24
0.24
0.07
50.
078
0.04
80.
038
0.18
0.16
0.03
3
AR21
8
3.17
29a
“---
i.84
1.77
2.10
2.10
0.27
0.28
0.09
70.
096
0.04
00.
030
0.18
0.16
0.01
6(0
.043
)(0
.059
)
0.06
4
0.14
0.10
0.14
0.10
*Cer
tifi
edva
lues
forPO
arein
erro
r.25
AR21
9
6.24
6.7K
“.-”
2.81
2.66
3.60
3.57
0.45
0.46
0.09
10.
087
0.05
30.
041
0.24
0.21
0.03
8
AR22
0
4.42
aaA~
.A.
1.Y
3
1.88
2.96
2.96
0.09
0.09
0.07
10.
074
0.01
90.
014
0.21
0.20
0.01
1(0
.102
)(0
.087
)
0.14
0.09
0.14
0.10
TABL
E8.
P05
fnAs
h6
Cmpa
riso
nof
PCAve
rsus
lpha
Reso
urce
sAn
alys
es
Samp
le
AR11
4
AR21
3
AR21
6
AR21
7
AR21
8
AR21
9
AR22
0
AR77
4
AR77
8
AR77
9
(wei
ght,
%)
Cer
tifi
ed*
PC
A(A
lph
aR
eso
urc
es)
0.34
0.44
0.39
0.71
0.22
0.46
0.50
0.63
0.19
0.78
0.27
0.72
0.11
0.87
0.16
0.20
0.46
0.48
0.10
0.18
*Ori
gina
lva
lues
foun
dto
bein
erro
r;re
vise
dva
lues
ente
red
here
.
**La
terce
rtif
iedva
lues
rece
ived
from
Alph
aRe
sour
cesre
pre-
sent
ingre
sult
sfr
omagr
eate
rnu
mber
ofpa
rtic
ipat
ing
labo
rato
ries
.
)T
A6L
E9.
Lin
ear
Reg
ress
ion
Dat
afo
r5e
vera
lO
xid
esan
dC
hlo
rid
ein
whol
eCo
al
)
sio2
A120
3‘e
2Q3
CaO
Mgo
S03
Na20
K20
Ti02
‘2°5
cl-
Corr
eiat
ionfa
ctor
-..
.AU
.Y03
Yn
“n””
U.Y
U*O
0.97
190.
9760
0.91
$2G
.987
~~.
~~~~
~.~~
~~n
on
lcV
.OU
IUn
n>n
nU
.7JU
Vn
nn
oc
V.3
YO
J
S1op
e4.
3018
1.28
623.
1859
0.47
350.
1396
0.15
990.
0751
o.i9
340*
Q972
(3.0
710
0.22
48
Inte
rcep
t-0
.852
2-0
.116
4-0
,889
8-0
.122
4-0
,120
1-1
.208
7-0
.058
0-0
.013
9-0
.022
80.
0099
-0.0
166
Stan
dard
devi
atio
n,%
0.20
0.11
0.28
0.05
0.04
0.55
0.01
20.
030.
030.
006
0.00
4
Aver
age
erro
r,%
0.16
0.08
0.22
0.05
0.03
0.44
0.00
90.
020.
020.
004
0.00
3
Numb
erof
samp
les
1921
1919
2222
2222
2210
13
TABL
E10
.Mu
ltip
leRe
gres
sion
Coef
fici
ents
forSe
lect
edO
xid
esin
Whol
eC
oal
Si02
“2°3
‘e20
3Ca
OS0
3S0
3K2
0Ti
02
(All
)(L
ow)
Corr
elat
ionfa
ctor
Stan
dard
deviat
ion,
%
Aver
age
erro
r,%
Inte
rcep
t
x — X2
— Si02
A12
03
Fe20
3
CaO
S03
K20
Ti02
0.99
80
0.14
0.12
0.44
4919
0.44
0835
0.05
1240
-0.0
4211
1
-0.0
0042
8
0.00
7096
0.00
0354
-0.0
0591
2
---
0.99
42
0.08
0.06
0.15
736
0.35
579
-0.0
1096
8
0.02
4456
.
0.00
1232
0.01
1426
---
-0.0
0781
7
0.01
0949
0.99
59
0.11
0.08
-0.0
1771
4
0.03
5487
0.00
0259
0.00
5010
0.00
2309
—
0.00
0746
0.00
0360
-0.0
0208
7
-0.0
0609
5
0.99
86
0.02
0.02
-0.0
3845
5
0.22
6151
0.02
5597
0.01
6752
0.01
2354
0.00
1971
-0.0
0045
3
-0.0
1012
1
-0.0
2940
0
0.99
39
0.38
0.28
-0.3
1241
1
0.11
0916
---
0.00
4766
0.01
7776
0.00
0931
..-
.
-0.0
0137
2
-0.0
2021
8
0.98
92
0.17
0.14
0.07
581
0.14
524
---
0.01
0012
0.01
8700
0.00
0258
-0.0
0318
2
—
-0.0
0359
4
-0.0
3666
8
0.99
50
<().
01
0.01
0.00
7959
0.00
8172
---
0.00
2205
-0.0
0159
1
0.00
0136
0.00
0899
0.00
0074
0.00
0507
0.99
30
<0.0
1
0.01
-0.0
1720
9
0.02
5449
-0.0
0241
6
0.00
2623
-0.0
0044
4
0.00
0052
0.00
1223
0.00
0118
-0.0
0048
8
—
~an
d~z
areth
ere
gres
sion
coef
fici
ents
ofth
ean
alyt
e.
---te
rmre
ject
edby
prog
ram.
repe
atof
X2te
rm.
——
))
)TA
BLE11
.Li
near
Regr
essi
onDa
tafo
rS0
3
Samp
le
AR11
4AR
213
/InO
lcn
Kcl
>
AR21
6
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
172
AR77
3AR
774
AR17
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
‘I26
.62
20.1
8~~
.~~
22.7
923
.77
45.0
457
.51
79.5
064
.90
83.1
8
18.1
024
.42
11.9
316
.70
24.4
0
27.2
122
.72
32.0
931
.02
41.2
8
55.1
460
.66
(wei
ght,
%)
Cert
ifie
d
2.28
1.50
1lK
,.I.
J2.
483.
08
6.40
9.25
10.8
09.
0512
.70
1.48
2.08
0.98
1.58
2.23
3.23
3.53
3.58
4.00
5.15
7.25
7.95
Corr
elat
ionfa
ctor
S1op
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XRF
3.05
2.02
nah
“..7 2.44
2.59
5.99
7.99
11.5
09.
1712
.09
1.69
2.70
0.70
1.46
2.69
3.14
2.43
3.92
3.75
5.39
7.61
8.49
0.98
710.
1599
-1.2
087
0.55
0.44
A
*.77
+0.5
2n
71
–.”.
.!
-0.0
4-0
.49
-0.4
1-1
.26
*.70
W.12
-0.6
1
4.21
G.62
-0.2
8-0
.12
*.46
-0.0
9-1
.10
m.34
-0.2
5~.
24
u3.3
6@.
54
)TA
BLE12
.Mu
ltip
leRe
gres
sion
Data
forS0
3
Samp
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8
AR21
9AR
220
AR38
0AR
510
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6
AR77
7AR
778
AR
779
AR
780
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
2.28
1.50
1.15
2.48
3.08
6.40
9.25
10.8
09.
0512
.70
1.48
2.08
0.98
1.58
2.23
3.23
3.53
3.58
4.00
5.15
7.25
7.95
XRF
2.82
1.66
0.90
2.30
2.79
5.22
8.93
10.6
39.
1812
.68
1.57
2.67
0.75
1.58
2.25
3.53
3.37
3.61
3.80
5.63
7.57
8.31
Stan
dard
devi
atio
n0.
38Av
erag
eer
ror
0.28
A
+0.54
+o.1
6
-0.2
5-0
.18
-0.2
9
-1.1
8
-0.3
2-0
.17
+0.1
3-0
.02
+0.0
9+0
.59
-0.2
30.
00M
.02
+0.3
0-0
.16
@.0
3-0
.20
+0.4
8
+0.3
24.
36
TABL
E13
.Mu
ltip
leRe
gres
sion
Data
forS0
3
(Inc
lude
son
lysa
mple
swi
thle
ssth
an5.
15%S0
3)
(wei
ght,
%)
Samp
le
AR11
4.r
.Q’l
-/i
KLIJ
AR21
5AR
216
AR21
7
AR77
1
AR77
2AR
773
AR77
4AR
775
AR77
6AR
777
AR77
8AR
779
AR78
0
Cert
ifie
d
2.28
.rn
1.3U
1,15
2.48
3.08
1.48
2.08
0.98
1.58
2.23
3.23
3.57
3.58
4.00
5.15
XRF
2.57
1“,
1.+
1
~=
17
2.23
2.91
1.29
2.39
1.01
1.83
2.10
3.27
3.47
3.66
3.92
5.12
Stan
dard
devi
atio
n0.
17Av
erag
eer
ror
0.14
A
+o.2
9A.-
-U,U
Y+
Q*o
~
-0.2
5-0
.17
-0.1
9+0
.31
+0.0
3+0
.25
-0.1
3
+0,04
-0,1
0+0
.08
-0.0
8-0
.03
))
)TA
BLE14
.Li
near
Regr
essi
onDa
tafo
rSi
02
Samp
le
AR11
4AR
213
AR21
5*AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3*
AR77
4AR
775
AR77
6AR
777*
AR77
8AR
779
AR78
0
AR78
1
AR78
2
‘I
1.38
871.
0219
0.41
211.
1480
1.53
97
0.95
241.
6330
1.19
581.
2981
0.87
56
1.04
241.
2330
0.40
13
1.08
300.
9989
1.35
562.
4864
1.11
911.
0588
0.97
01
1.76
480.
6497
(wei
ght,
%)
Cert
ifie
d
5.18
3.46
1.70
3.77
5.84
3.24
6.25
4.45
4.97
3.20
3.35
4.43
1.51
4.15
3.16
4.67
12.2
03.
953.
543.
36
6.79
2.10
Corr
elat
ionfa
ctor
Slop
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XRF
5.12
3.54
4.09
5.77
3.24
6.17
4.29
4.73
2.91
3.63
4.45
3.81
3.44
4.98
3.96
3.70
3.32
6.74
1.94
0.98
594,
3018
-0.8
522
0.20
0.16
A
-0.0
6+o
.08
+0.3
Z-0
.07
0.00
-0.0
8-0
.16
-0.2
4-0
.29
+o,2
8
+0.0
2
-0.3
4+0
.28
+0.3
1
+0.0
1+o
016
-0,0
4
-0.0
5-0
.16
TABL
E15
.Mu
ltip
leRe
gres
sion
Data
forSi
Op
Samp
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6
AR77
7AR
778
AR77
9AR
780
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
5.18
3.46
1.70
~.~~
5.84
3.24
6.25
4.45
4.97
3.20
3.35
4.43
1.51
4.15
3.16
4.67
12.2
03.
953.
54
3.36
6.79
2.10
XRF
4.97
3.49
1.54
3.94
5.63
3.25
6.36
4.39
4.85
3.02
3.54
4.29
1.51
3.95
3,35
4.74
12.2
14.
013.
67
3.37
6.89
2.28
Stan
dard
devi
atio
n0.
14Av
erag
eer
ror
0.12
A -0.2
1m.
03-0
.16
+0.?
7-0
.21
@.ol
+().
11
-0.0
6-0
.12
-0.1
8
+().
19
-0.1
40.
00-0
.20
+().
19
+0.0
7
+0.0
1+0
.06
+0.1
3
@.ol
+0.1
0
+o.1
8
mot
used
inli
near
regr
essi
on.
TABL
E16
.Li
near
Regr
essi
onDa
tafo
rA1
203
Samp
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777*
AR77
8AR
779
AR78
0
AR78
1AR
782
‘I2.
1517
1.53
330.
7747
~.g:
~~
2.22
14
1.47
492.
1371
1.51
601.
7322
1.30
07
1.54
871.
9696
0.81
061.
2165
1.73
46
2.27
652.
7067
1.58
041.
3828
1.29
54
2.05
781.
0535
(wei
ght,
%)
Cert
ifie
d
2.87
1.79
0.93
2.25
2.79
1.77
2.66
1.88
2.28
1.73
1.78
2.32
0.87
1.44
1.91
2.74
4.38
1.91
1.64
1.58
2.54
1.23
Corr
elat
ionfa
ctor
Slop
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XRF
2.65
1.86
0.88
2.38
2.74
1.78
2.63
1.83
2.11
1.56
1.88
2.42
0.93
1.45
2.11
2.81
1.92
1.66
1.55
2.53
1.24
0.98
461.
2862
-0.1
164
0.11
0.08
A
-0.2
2W.
07-0
.05
%.13
-0.0
5
W.ol
-0.0
3-0
.05
-0.1
7-0
.17
@lo
+0.1
0~.
06+0
,01
W.20
N.07
+0.0
1*.
02-0
.03
-0.0
1+0
.01
TA
BL
E17
.M
ult
iple
Reg
ress
ion
Dat
afo
rA
1203
Samp
le
AR11
4AR
213
AR21
5AR
2i6
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
2.87
1.79
0.93
~.25
2.79
7.77
2.66
1.88
2.28
1.73
1.78
2.32
0.87
1.44
1.91
2.74
4.38
1.91
1.64
1.58
2.54
1.23
XRF
2.68
1.82
0.92
2.31
2.71
1.75
2.88
1.86
2.22
1.63
1.79
2.32
0.95
1.45
2.03
2.77
4.35
1.92
1.59
1.55
2.60
1.22
Stan
dard
devi
atio
n0.
08Av
erag
eer
ror
0.06
A
-0.1
9+0
.03
-0.0
1+0
.06
-0.0
8
-0.0
2
*.22
-0.0
2-0
.06
-0.1
0
+0.0
10,
00+0
.08
W.ol
+0.1
2
+0.0
3
-0.0
3+O
.O1
-0.0
5-0
.03
fl.0
6-0
.01
*Not
used
inli
near
regr
essi
on.
)
)TA
BLE18
.Li
near
Regr
essi
onDa
tafo
rFe
203
Samp
le
AR11
4A
D91
2n
,.L
,.J
AR21
5*AR
216
AR21
7
AR21
8
AR21
9AR
220
AR38
0AR
510
AR77
1AR
772
AR77
3*AR
774
AR77
5
AR77
6AR
777*
AR77
8AR
779
AR78
0
AR78
1AR
782
‘I
0.61
44n
7nK
l“.
,””.
0.22
310.
4206
0.48
44
0.93
151.
2633
1.11
951.
0735
1.87
39
0.70
910.
7184
0.22
900.
4928
0.46
54
0.67
190.
7281
0.60
820.
8521
1.31
12
0.88
831.
0134
(wei
ght,
%)
Cert
ifie
d
0.96
1nl
..”.
0.35
0.68
0.96
2.10
3.57
2.96
2.81
5.23
1.00
1.11
0.32
0.75
0.76
1.24
2.11
1.12
1.62
2.62
2.04
2.22
Corr
elat
ionfa
ctor
Slop
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XRF
1.07
~.~~
0.45
0.65
2.08
3.13
2.68
2.53
5.08
1.37
1.40
0.68
0.59
1.25
1.05
1.82
3.29
1.94
2.34
0.97
193.
1849
;.~;
98
0:22
A
+0.11
+o=~
~
-0.2
3-0
.31
-0.0
2
-0.4
4-0
.28
-0.2
8-0
.15
*.37
*.29
-0.0
7-0
.17
4.01
-0.0
7a.
20*.
67
-0.1
0@.
12
TA8L
E19
.Wl
tipl
eRe
gres
sion
Data
forFe
203
Sam
ple
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8
AR21
9AR
220
AR38
0AR
510
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
0.96
1.01
0.35
0.68
0.96
2.10
3.57
2.96
2.81
5.23
1.00
1.11
0.32
0.75
0.76
1.24
2.11
1.12
1.62
2.62
2.04
2.22
XRF
1.13
0.97
0.29
0.69
0.93
1.78
3.47
2.85
2.75
5.25
0.96
1.24
0.28
0.78
0.75
1.31
2.16
1.15
1.58
2.76
2.10
2.37
Stan
dard
devi
atio
n0.
11Av
erag
eer
ror
0.08
A
io.1
7-0
.04
-0.0
6U3
.ol
-0.0
3
-0.3
2-0
.10
-0.1
1-0
.06
a.02
-0.0
4W.
13-0
.04
a.03
-0.0
1
a.07
W.05
W.03
-0.0
4@.
14
@.06
W.15
*Not
used
inli
near
regr
essi
on.
TABL
E20
.Li
near
Regr
essi
onDa
tafo
rCa
O
Samp
le
AR11
4AR
213
..-7
,*n
ficl
a-
AR
21
6
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
JAR
772
AR77
3*AR
774
AR77
5
AR77
6AR
777*
AR77
8AR
779
AR78
0
AR78
1AR
782
RI
0.84
230.
5578
Q91
cnC
.ala
u
0.81
630.
4276
0.90
930.
9945
0.35
192.
2490
0.28
07
0.48
100.
8945
2.27
800.
9229
0.85
90
1.92
67
3.27
860.
7489
0.59
850.
4090
0.52
340.
5316
(wei
ght,
%)
Cert
ifie
d
0.24
0.10
nQ
Ov.
”, 0.20
0.12
0.28
0.46
0.09
1.02
0.08
0.10
0.25
0.78
0.26
0.22
0.76
2.01
0.21
0.12
0.10
0.17
0.15
Corr
elat
ionfa
ctor
S1op
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XR
F
0.28
0.14
0.26
0.08
0.31
0.35
0.04
0.94
0.01
0.10
0.30
0.31
0.28
0.79
0.23
0.16
0.07
0.12
0.13
0.97
600.
4735
-0.1
224
0.05
0.05
A
W.04
a.04
@.06
-0.0
4
M.0
3-0
.11
-0.0
5-0
.08
-0.0
7
0.00
m.0
5
M.0
5ti
.06
4.03
M.0
2M
.04
-0.0
3
-0.0
5-0
.02
TABL
E21
.Mu
ltip
leR
egre
ssio
nDa
tafo
rCa
O
Samp
le
AR11
4AR
213
AR~~
~
AR21
6AR
217
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
0.24
0.10
~=~g
0.20
0.12
0.28
0.46
0.09
1.02
0.O
B
0.10
0.25
0.78
0.26
0.22
0.76
2.01
0.21
0.12
0.10
0.17
0.15
XRF
0.26
0.12
~.~
g
0.21
0.08
0.27
0.42
0.09
1.03
0.09
0.10
0.20
0.81
0.27
0.25
0.77
2.01
0.23
0.13
0.12
0.15
0.17
Stan
dard
devi
atio
n0.
02Av
erag
eer
ror
0.02
A
@.02
4.02
-~.~
~
W.ol
-0.0
4
-0.0
1-0
.04
0.00
@.ol
W.ol
0.00
-0.0
5w.0
3M
.01
w.0
3
@.0
10.
00w
.02
W.ol
@.0
2
-0.0
2M
.02
*Not
used
inli
near
regr
essi
on.
))
,)
)TA
BLE22
.Li
near
Regr
essi
onDa
tafo
rMg
O
Samp
le
AR11
4AR
213
flQ
91C.
“,.
L.”
AR21
6AR
217
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6
AR77
7AR
778
AR77
9AR
780
AR78
1AR
782
RI
1.30
801.
1731
g.fi
~~~
1.09
301.
2621
1.78
621.
8002
1.80
351.
8494
1.75
86
1.16
861.
3445
1.62
461.
3446
1.07
88
2.29
503.
9168
1.20
641.
3606
1.45
87
2.06
601.
3261
(wel
gnt,
%)
Cert
ifie
d
0.08
0.06
0=18
0.05
0.07
0.10
0.09
0.07
0.11
0.04
0.06
0.08
0.17
0.09
0.05
0.20
0.47
0.06
0.07
0.07
0.14
0.03
~O~l
atio
nfa
ctor
Inte
rcep
tSt
anda
rdde
viat
ion
Aver
ageer
ror
XR
F
0.06
0.04
n.11
0.03
0.06
0.13
0.13
0.13
0.14
0.12
0004
0.07
0.11
0.07
0.03
0.20
0.43
0.05
0.07
0.08
0.17
0.07
0.91
420.
1396
-0.1
201
0.04
0.03
A
-0.0
2-0
.02
-0.0
7-0
.02
-0.0
1
a.03
N.04
@.06
W*O3
u3.0
8
-0.0
2-0
.01
-0.0
6-0
.02
-0.0
2
0.00
-0.0
4-0
.01
0.00
a.0
1
w.0
34.
04
TABL
E23
.Li
near
Regr
essi
onD
ata
for
K20
Sai
np
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR7B
0
AR78
1AR
782
‘I
1.00
211.
0847
0.19
070.
7937
1.23
98
0.97
561.
0829
1.04
531.
1315
0.60
03
1.07
820.
9594
0.20
831.
1306
0.64
87
1.19
460.
8138
0.77
631.
2930
0.90
17
1.74
380.
3557
(wei
ght,
%)
Cer
tifi
ed
0.17
0.16
0.02
0.12
0.21
0.16
0.21
0.20
0.23
0.13
0.16
0.16
0.03
0.17
0.09
0.21
0.22
0.13
0.20
0.17
0.37
0.06
Corr
elat
ionfa
ctor
Slop
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XRF
0.18
0.20
0.02
0.14
0.23
0.17
0.20
0.19
0.20
0.10
0.19
0.17
0.03
0.20
0.11
0.21
0.14
0.14
0.24
0.16
0.32
0.05
0.93
340.
1934
-0.0
139
0.03
0.02
A
tool
+0 .04
---
u.U
u%
.02
a*02
+0.
01-0
.01
-0.0
1-0
.03
-0.0
3
+0.0
3io
.ol
0.00
a.03
a.02
0.00
-0.0
8W.
olW.
04-0
.01
-0.0
5-0
.01
TABL
E24
.M
ult
iple
Reg
ress
ion
Dat
afO
rK
20
Sam
ple
AR11
4AR
213
..a.
,.N
K<1
3AR
~~~
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
0.17
0.16
-..
U.U
L0
81
Z
0.21
0.16
0.21
0.20
0.23
0.13
0.16
0.16
0.03
0.17
0.09
0.21
0.22
0.13
0.20
0.17
0.37
0.06
XRF
0.17
0.16
...
U.U3
0=12
0.21
0.16
0.23
0.20
0.23
0.12
0.16
0.16
0.03
0.17
0.09
0.21
0.22
0.12
0.20
0.16
0.36
0.06
A 0.00
0.00
.,-.n.
W.ul
0:00
0.00
0.00
W*O2
0.00
0.00
-0.0
1
0.00
0.00
0.00
0.00
0.00
0.00
0.00
-0.0
10.
00-0
.01
-0.0
1
0.00
0.01
Stan
dard
devi
atio
n.
Aver
ageer
ror
<0.0
1
N o
))
)TA
BLE25
.Li
near
Regr
essi
onDa
tafo
rTi
02
Sam
ple
AR11
4AR
~~~
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
‘I
1.78
981.~~
~u
0.93
601.
6516
1.54
40
1.26
021.
3699
1.06
981.
0667
0.86
50
1.76
841.
6943
0.99
131.
0889
1.56
21
1.52
861.
9443
1.26
480.
8897
1.06
55
1.40
97
0.68
48
(wei
ght,
%)
Cer
tifi
ed
0.14
0.11
0.06
0.12
0.13
0.10
0.14
0.10
0.10
0.08
0.11
0.12
0.06
0.07
0.11
0.12
0.25
0.09
0.06
0.08
0.14
0.04
~O~l
atio
nfa
ctor
Inte
rcep
tSt
anda
rdde
viat
ion
Aver
ageer
ror
XRF
0.15
0.14
0.07
0.14
0.13
0.10
0.11
0.08
0.08
0006
0.15
0.14
0.07
0.08
0.13
0.13
0.17
0.10
0.06
0.08
0.11
0.04
0.80
160.
0972
-0.0
228
0.03
0.02
A
@.ol
a.0
3@.
ol@
.02
0.00
0.00
-0.0
3-0
.02
-0.0
2-0
.02
@.0
4+0
.02
+0.
01N
.01
+0.0
2
@.0
1-0
.08
+0.0
10.
000.
00
-0.0
3
0.00
)TA
BLE26
.Wl
tipl
eRe
gres
sion
Data
for
Ti02
Samp
le
AR11
4AR
213
AR21
5AR
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR77
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
(wei
ght,
%)
Cert
ifie
d
0.14
0.11
0.06
0.12
0.13
0.10
0.14
0.10
0.10
0.08
0.11
0.12
0.06
0.07
0.11
0.12
0.25
0.09
0.06
0.08
0.14
0.04
Stan
dard
devi
atio
nXRF
0.14
0.11
0.06
0.1.
20.
13
0.10
0.14
0.10
0.10
0.08
0.11
0.13
0.06
0.08
0.11
0.13
0.25
0.10
0.05
0.08
0.14
0.05
A 0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
4.01 0.00
+0.
010.
00
+0.
010.
00+
0.01
-0.0
10.
00
0.00
+0.
01
0.01
Aver
ageer
ror
<0.0
1
TABL
E27
.Li
near
Regr
essi
onDa
tafo
rNa
20
Sam
ple
AR11
4AR
213
.n*1
Cm
zla
A!?
216
AR21
7
AR21
8AR
219
AR22
0AR
380
AR51
0
AR77
1AR
772
AR77
3AR
774
AR71
5
AR77
6AR
777
AR77
8AR
779
AR78
0
AR78
1AR
782
‘I
1.44
241.
2430
cC
CA
9O
.ao
yc
1.26
411.
1452
1.30
981.
3406
0.97
221.
5751
0.91
86
1.20
221.
6709
6.38
731.
5409
1.11
94
2.32
081.
3477
1.44
660.
9246
0.97
75
1.61
130.
9628
(wei
ght%)
Cert
ifie
d
0.03
80.
025
~,Q
~
0.03
80.
025
0.03
00.
041
0.01
40.
049
0.03
2
0.03
20.
051
0.41
0.05
50.
014
0.11
80.
055
0.04
30.
035
0.02
5
0.07
20.
019
~O~l
atio
nfa
ctor
Inte
rcep
tSt
anda
rdde
viat
ion
Aver
ageer
ror
XRF
0.05
00.
035
g.~~
0.03
70.
028
0●04
00.
043
0.01
50.
060
0.01
1
0.03
20.
067
0.42
0.05
80.
026
0.11
60.
043
0.05
10.
011
0.01
5
0.06
30.
014
:.;;
;:
::;;
;0
0:00
9
A
@.o1
2W.
olo
4.!!
20-0
.001
W.00
3
W.ol
o@.
oo2
Wool
to.o
ll-0
.021
0.00
0@.
016
M.ol
oN
.003
4.01
2
-0.0
02-0
.012
@.0
08-0
.024
-0.0
10
-0.0
09-0
.005
TABL
E28
.Li
near
Regr
essi
onOa
tafo
rP2
05
Samp
le
AR11
4AR
213
AD
716
.“.
-,.,
AR21
7AR
218
AR21
9
AR22
0AR
774
AR71
8AR
779
(wei
ght,
%)
‘IPC
A
0.67
50.
033
0.65
90.
027
n?G
l“.
””,
nn1
7w.”,
,0.
752
0.05
20.
334
0.01
6
0.57
50.
038
0.30
60.
011
0.30
10.
011
0.67
00.
036
0.26
50.
007
Corr
elat
ionfa
ctor
Slop
eIn
terc
ept
Stan
dard
devi
atio
nAv
erag
eer
ror
XR
F
0.03
8
0.03
7n
nl~
“.”,-
0.04
30.
014
0.03
1
0.01
20.
011
0.03
80.
009
0.93
040.
0710
0.00
990.
006
0.00
4
A
+0.0
05+(
).01
0_~
.g~~
-0.0
09-0
.002
-0.0
07+0
.001
0.00
0W.
002
U3.0
02
)
PCA X!esearch and Development Bulletin 23
3 “-6sg $8--O- . . . . do000
w Tt-f”)‘Dhcu
$
--c-v I-NNNN
Z%ZZ%
c + *
24 Coal Charac~erization b.v X-Ray Speclrometry
(IJ
I Si02
*
7.58
5.60
6.27
8.40
5.20
8.91
6.53
5.77
5.91
6.11
5.38
9.51
7.06
4.76
5.65
5.26
3.52
6.69
7.40
13.4
2
2.20
2.17
[2Si
02
57.4
631
.36
39.3
170
.56
27.0
4
79.3
942
.64
33.2
934
.93
37.3
3
28.9
290
.36
49.8
322
.70
31.8
7
27.6
212
.38
44.7
854
.70
180.
10
4.84
4.71
)TA
BLEA-
1.Mu
ltip
leRe
gres
sion
Data
forSi
lica
(Si0
2)
(Based
onLucas-Tooth
andPy
neeq
uati
on)
[1Si
02”1
A120
3)
36.2
319
.04
27.0
941
.66
17.1
1
42
.32
21
.94
17
.71
15
.96
21
.51
20.5
243
.40
26.8
413
.63
18.8
8
14.7
08.
0028
.14
37.0
578
.91
3.73
3.82
*ISi
02=co
unts
perse
cond
/100
0
I1Si
02“1
Fe20
3)
154.
0313
0.54
87.3
413
5.07
160.
52
371.
9024
0.83
161.
9696
.04
123.
06
82.8
227
9.39
250.
7129
5.36
132.
19
227,
5511
7.77
157.
6216
4.19
321.
41
16.29
16.34
(1S
i02*
1CaO
)
8.34
3.86
6.14
2.69
6.08
11.6
72.
943.
587.
095.
87
6.13
6.60
21.0
61.
773.
60
2.85
2.48
6.20
18.9
058
.38
6.82
6.55
(1S
i02e
1S03
)
161.
0891
.06
120.
2616
1.28
195.
00
423.
0542
0.20
147.
6583
.04
162.
28
105.
6942
8.33
374.
4332
3.89
90.5
8
192,
2918
9.22
141.
0517
2.30
257.
40
25.1
521
.85
[1Si
02”1
K20)
48.9
739
.26
32.0
467
.45
32.8
1
62.2
844
.01
48.1
843
.20
30.5
5
22.4
610
6.73
51.4
318
.42
38.9
8
30.3
58.
0240
.96
57.2
070
.32
2.73
2.91
(1Si
02”1
Ti02
)
35
.47
24
.64
27
.15
33
.94
17
.16
31
.99
18
.35
8.2
51
6.8
42
0.2
2
21
.96
35
.02
19
.68
10
.77
25
.81
14
.48
6.2
32
9.6
12
9.3
86
8.1
7
5.4
45
.62
5.18
3.46
3.77
5.84
3.24
6.25
4.45
3.54
4.15
3.95
3.16
6.79
4.97
3.20
3,35
3.36
2.10
4.43
4.67
12.2
0
1.70
1.51
TABL
EA-
2.hl
tipl
eRe
gres
sion
Dat
afo
rA
lum
ina
(A12
03)
1A12
03*
4.78
3.40
4.32
4.96
3.29
4.75
3.36
3.07
2.70
3.52
3.82
4.57
3.80
2.86
3.34
2.80
2.27
4.21
5.01
5.88
1.68
1.76
2 “2°3
22.8
511
.56
18.6
624
.60
10.8
2
22.5
611
.29
9.42
7.29
12.3
9
14.5
620
.85
14.4
68.
1811
.18
7.82
5.17
17.6
825
.09
34.5
7
2.82
3.10
1A12
03”1
Si02
)
36.2
319
.04
27.0
9;;
.;:
.
42.3
221
.94
17.7
115
.96
21.5
1
20.5
243
.40
26.8
413
.63
18.8
8
14.7
08.
0028
.14
;:.;
;.
3.73
3.82
(Bas
edon
Luca
s-To
othan
dP~
eeq
uati
on)
1A12
03”1
Fe20
3)
97.1
379
.25
60.1
879
.76
101.
56
198.
2712
3.92
86.1
743
.88
70.8
9
58.7
713
4.20
135.
041;
:.;;
.
121.
1176
.11
99.0
411
1.20
140.
83
12.3
313
.25
[1A
1203
*1C
aO)
5.26
2.97
4.23
2.83
3.85
6.22
1.51
1.90
3.24
3.38
4.35
3.17
11.35
1.06
2.13
1.52
1.60
3.90
12.8
025
.58
5.16
5.32
[*A1
203”
1S03
)
101.
5855
.28
82.8
695
.23
123.
38
225.
5321
6.22
78.5
637
.94
93.4
9
75.0
020
5.74
201.
6719
4.44
53.6
6
102.
3512
2.28
88.6
311
6.70
112.
78
19.0
317
.72
[‘A1
203*1K
20)
30.8
823
.83
22.0
839
.83
20.7
6
33.2
022
.65
25.6
319
.74
17.6
0
15.9
451
.27
;<.;
:
23:0
9
16.1
55.
1825
.73
:1.:
!.
2.07
2.36
[1A1
203*
1Ti0
2)
22.3
714
.96
18.7
119
.96
10.8
6
17.0
59.
447.
157*
7O11
.65
;;.;:
10:6
06.
4715
.29
7.71
4.03
18.6
119
.90
29.8
7
4.12
4.56
‘A12
03
2.87
1.79
2.25
2.79
1.77
2.66
1.88
1.64
1.44
1.91
1.91
2.54
2.28
1.73
1.78
1.58
1.23
2.32
2.74
4.38
0.93
0.87
*IA1
203=co
unts
per
seco
nd/1
000
)
)
1Fe2
03*
20.3
223
.31
13.9
316
.08
30.8
7
41.7
436
.88
28.0
716
.25
20.1
4
15.4
029
.39
35.5
262
.00
23.4
2
43.3
033
.47
23.5
522
.20
23.9
5
7.34
7.53
12
‘e20
3
412.
9054
3.36
194.
0525
8.57
952.
96
1742
.23
1360
.13
787.
9226
4.06
405.
62
237.
1686
3.83
1261
.46
3;::
.:;
.
1874
.98
1120
.11
554.
7449
2.88
573.
60
53.8
856
.70
TA
BL
EA-3
.ti
ltip
leRe
gres
sion
Data
forFe
rric
Oxid
e(F
e203)
1Fe2
0301
Si0
2)
154.
0313
0.54
87.3
413
5.07
160.
52
371.
9024
0.83
161.
9696
.04
123.
06
82.8
227
9.39
250.
7129
5.36
132.
19
227.
5511
7.77
157.
6216
4.19
321.
41
16.2
916
,34
*IFe
203=co
unts
perse
cond
/100
0
:1Fe
203”
1A12
03)
97.1
379
.25
60.1
879
.76
101.
56
198.
2712
3.92
86.1
7;;
.::
.
58.7
713
4.20
135.
0417
7.32
78.3
1
121.
1176
.11
99.0
411
1.20
140.
83
12.3
313
.25
1Fe2
03”1
CaO)
22.3
516
.08
1;.:
;
36:1
2
54.6
816
.60
17.4
019
.50
19.3
3
17.5
620
.40
105.
9823
.06
14.9
2
23.4
723
.56
21.8
356
.75
104.
18
22.5
322
.74
:1F
e203
“1S
03)
431.
8037
9.02
267.
1830
8.74
1157
.63
1981
.82
2373
.23
718.
3122
8.31
534.
92
302.
6613
24.3
318
83.9
342
15.1
337
5.77
1584
,47
1799
.64
496.
4351
7.26
459.
36
83.1
675
.83
‘Fe2
03”1
K20
)
i3i.
2i16
3.40
71.1
812
9.12
194.
79
291.
7624
8.57
234.
3811
8.79
100.
70
64.3
333
0.00
258.
7523
9.69
161.
70
250.
0676
.27
144.
1417
1.70
125.
50
9.03
10.0
9
~1Fe
203”
1Ti0
2)
95.1
010
2.56
60.3
264
.96
101,
87
149.
8510
3.63
65.4
046
.31
66.6
6
62
.88
10
8.2
899
.02
140.
1810
7.09
119.
3459
.27
104.
2288
.20
121.
67
17.9
819
.50
cFe2
03
:.:;
0:68
0.96
2.10
3.57
2.96
1.62
0.75
1.12
0.76
2.04
2.81
5.23
1.00
2.62
:.;;
1:24
2.11
0.35
0.32
TABL
EA-
4.Mu
ltip
leRe
gres
sion
Data
forLi
me(C
aO)
N Oa
I CaO
*
1.10
0.69
0.98
0.57
1.17
1.31
0.45
0.62
1.20
0.96
1.14
0.69
2.98
0.37
0.64
0.54
0.70
0.93
2.56
4.35
3.07
3.02
2Ca
O
1.21
0.48
0.96
0.32
1.37
1.72
0.20
0.39
1.44
0.92
1.30
0.48
8.9C
0.14
0.41
0.25
0.5C
0.86
6.5:
18.9
2
9.4;
9.1;
*CaO
”]Si
02)
8.34
3.86
6.14
2.69
6.08
11.6
72.
943.
587.
095.
87
6.13
6.60
21.0
61.
773.
60
2.85
2.48
6.20
18.9
058
.38
6.82
6.55
~ lC
aO”1A1
203)
5.26
2.97
4.23
2.83
3.85
q.:;
1:90
3.24
3.38
4.35
3.17
11.3
51.
062.
13
1.52
1.60
3.90
12.8
025
.58
5.16
5.32
:1Ca
O”1F
e203)
22.3
516
.08
13.6
59.
1736
.12
54.6
816
.60
17.4
019
.50
19.3
3
17.5
620
.40
105.
9823
.06
14.9
2
23.4
723
.56
21.8
356
.75
104.
18
22.5
322
.74
[1Ca
O*1S
03)
23.3
811
.22
18.8
010
.94
43.8
8
62.2
028
.96
15.8
716
.86
25.5
0
22.4
031
.27
158.
28:;
.;;
.
19.8
337
.86
19.5
459
.55
83.4
3
34.7
830
.41
:1Ca
O”]K
20)
7.11
4.84
5.01
4.58
7.3a
9.16
3*O3
5.18
8.77
4.80
4.76
7.79
21.8
41.
444.
40
3.13
1.60
5.67
19.7
722
.79
3.78
4.05
(1Ca
O”1T
i02)
5.15
3.04
4.24
2.30
3.86
4.70
1.26
1.44
3.42
3.18
4.65
2.56
8.32
0.84
2.91
1.49
1.25
4.10
10.1
522
.10
7.52
7.82
c CaO
0.24
0.10
D.2
00.
120.
28
0.46
0.09
0.12
0.26
0.21
0.22
0.17
1.02
0.08
0.10
0.10
0.15
0.25
0.76
2.01
0.89
0.78
*1~a
o=
cou
nts
per
seco
nd/1
000
PCA Rt?search and Development Bulletin 29
,’--
al
l-l I
I -m I
.-
1
\uK00mm
TABL
EA-
6.Mu
ltip
leRe
gres
sion
Data
forPo
tass
iumOx
ide(K
20)
1K20
*I
6.46
7.01
5.11
8.03
6.31
6.99
6.74
8.35
7.31
5.00
4.18
1;.;: 3:87
6.91
5.78
2.28
6.12
7.73
5.24
1.23
1.34
12K2
0~
41.7
349
.14
26.1
164
.48
39.8
2
48.8
645
.48
69.7
253
.44
25.0
0
17.4
526
.07
53.0
914
.95
47.6
8
33.3
55.
1937
.45
59.8
127
.46
1.51
1.80
(1K2
0”1S
i02)
48.9
739
.26
32.0
467
.45
32.8
1
62.2
844
.01
48.1
843
.20
30.5
5
22.4
61::.;;
18:4
238
.98
30.3
58.
0240
.96
57.2
070
.32
2.73
2.91
1K20
”1A1
203)
30.8
823
.83
22.0
839
.83
20.7
6
33.2
022
.65
25.6
319
.74
17.6
0
15.9
451
.27
27.7
011
.06
23.0
9
16.1
55.
1825
.73
38.7
430
.81
2.07
2.36
~1K2
0*1F
e203
)
131.
2716
3.40
71.1
812
9.12
194.
79
291.
7624
8.57
234.
3811
8.79
100.
70
64.3
333
0.00
258.
7823
9.69
161.
70
250.
0676
.27
144.
1417
1.70
125.
50
9.03
10.0
9
:1K2
0”lC
aO)
7.11
4.84
5.01
4.58
7.38
9.16
3.03
5.18
8.77
4.80
4.16
7.79
21.8
41.
444.
40
3.13
1.60
5.67
19.7
722
.79
3.78
4.05
:1K2
0”1S
03)
137.
2811
3.98
98.0
115
4.18
236.
63
331.
8943
3.72
213.
6810
2.71
132.
80
82.0
950
5.92
386.
4726
2.84
110.
80
211.
3212
2.55
128.
9918
0.19
100.
50
13.9
413
.49
1K20
”1T
i02)
30.2
330
.84
22.1
332
.44
20.8
2
25.0
918
.93
19.4
620
.83
16.5
5
17.0
441
.36
20.3
18.
7431
.58
15.9
24.
0427
.08
30.7
326
.62
3.01
3.47
CK20
0.17
0.16
0.12
0.21
0.16
0.21
0.20
0.20
0.17
0.13
0.09
0.37
0.23
0.13
0.16
0.17
0.06
0.16
0.21
0.22
0.02
0.03
*IK2
0=co
unts
perse
cond
/100
0
)
‘) })
1Tf0
2*
4.68
4.40
4.33
4.04
3.30
3.59
2.81
2.33
;.;: .
4.08
3.68
2.79
2.26
4.57
2.76
1.77
:.::
5:08
2.45
2.59
[2Ti
02
21.9
019
.36
18.7
516
.32
10.8
9
12.8
97.
905.
438.
1210
.96
16.6
713
.57
7.77
5.11
20.9
1
7.60
3.14
19.5
815
.78
25.8
1
6000
6.71
TABL
EA-
7.~l
tipl
eRe
gres
sion
Data
forTi
tani
a(T
i02)
(1T
i02”
1Si0
2)
35.4
724
.64
27.1
5;:
.::
●
31.9
918
.35
8.25
16.8
420
.22
21.9
635
.02
19.6
810
.77
25.8
1
14.4
86.
2329
.61
29.3
868
.17
5.44
5.62
*ITi
O.=
cou
nts
per
seco
nd
/100
0
1Ti0
2”]A
1203
)
22.3
7;:
.;;
19:9
610
.86
17.0
59.
447.
157.
7011
.65
15.5
816
.82
10.6
26.
4715
.29
7.71
4.03
18.6
119
.90
29.8
7
4.12
4.56
[1T
i02”
1Fe2
03)
95.1
010
2.56
60.3
264
.96
101.
87
149.
8510
3.63
65.4
046
.31
66.6
6
62.8
810
8.24
99.0
214
0.18
107.
09
119.
3459
.27
104.
2288
.20
121.
67
17.9
819
.50
[1T
i02”
1CaO
)
5.15
3.04
4.24
2.30
3.86
4.70
1.26
1.44
3.42
3.18
4.65
2.56
8.32
0.84
2.91
1.49
1.25
4.10
10.1
522
.10
7.52
7.82
:1T
i02-
[S03
)
99.4
571
.54
83.0
477
.57
123.
75
170.
4518
0.82
59.6
240
.44
87.9
1
80.2
416
6.00
147.
8815
3.72
73.3
8
100.
85;:
.;;
92:5
797
.43
27.7
626
.08
(IT
i02*
*K20
)
30.2
330
.84
22.1
332
.44
20.8
2
25.0
918
.93
19.4
620
.83
16.5
5
17.0
4;:
.;;
8:74
31.5
8
15.9
24.
0427
.08
30.7
326
.62
3.01
3.47
‘Ti0
2
0.14
0.11
0.12
0.13
0.10
0.14
0.10
0.06
0.07
0.09
0.11
0.14
0.10
0.08
0.11
0.08
0.04
0.12
0.12
0.25
0.06
0.06
This publication is based on the facts, tests, and authorities stated herein.It is intended for the use of professional personnel competent to evaluate thesignificance and limitations of the reported findings and who will acceptresponsibility for the application <~fthe material it contains. The PortlandCement Association disclaims any and all responsibility for application ofthe stated principles or for the accuracy of any of the sources other than workperformed or information developed by the Association.
I______ ---. -__ —— — ---------------- -- ——----— — --------— ~---- --—- 1
uIII
KEYWORDS: analytical methods, chemical :analysis, chlorides, coal, coal analy- 1I
sis, spectrometry, X-ray fluorescence. II
ABSTRACT: Report of results of X-ray fluorescence procedure used formulti- 1I
element analysis of whole coal. Certified whole coal samples were ground, II
pressed, and analyzed in a vacuum with a Rigaku Model 3064X-ray spectrometer. 1Quantitative results ofadequate accuracy were obtained forthe oxides of 10ele- ~ments and for chlorine. Interelement corrections were necessary for ferric oxide 1
and sulfur trioxide—and for silica, alumina, and calcium oxide when lignite andII
subbituminous coals were used. Interelement corrections may also improve theII
accuracy for potassium oxide and titanium oxide. II
REFERENCE: J. L. Bernardi,(RD082.OIT), Portland Cement
Coal Characterization by X-Ray SpectrometryII
Association, 1983. IIII
—------------------ ----------- ------------------------- -- J
PCA R&D Ser. 1666
PORTLAND CEMENT mII ASSOCIATION
An organization of cement manufacturers to Improve and extend the uses of portland cement and <oncrete through ~cient, fic research, engineeric>g field work, and market development
Printed In U S.A.5420 Olcj Or(l).]rcj Kod(j, Skok((>, Illinois 60077-4121 RD082. OIT